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OBJECTIVE:To develop a method for simultaneous determination of 8 residual organic solvents in esomeprazole magnesium raw material,including ethanol,ethyl acetate,isopropylenzene,methanol,methylbenzene,2-phenyl-2-propanol,dichloromethane and acetonitrile.METHODS:Capillary GC was adopted.The determination was performed on HP-1 column by programmed temperature.The temperature of injector port was 220 ℃,with flame ionization detector at temperate of 250 ℃,using nitrogen as carrier gas,at the flow rate of 4.0 mL/min,with split ratio of 10∶1 and injection volume of 1 μL.RESULTS:The linear ranges of ethanol,ethyl acetate,isopropylenzene,methanol,methylbenzene,2-phenyl-2-propanol,dichloromethane and acetonitrile were 45.2-904 μg/mL(r=0.999 7),45.5-909 μg/mL(r=0.999 7),9.0-180 μg/mL(r=0.999 8),27.1-542 μg/mL(r=0.999 8),8.7-174 μg/mL(r=0.999 7),9.1-183 μg/mL(r=0.999 4),5.8-115 μg/mL(r=0.999 4),3.7-74 μg/mL(r=0.999 4),respectively.The quantitation limits were 4.5,3.0,1.4,2.7,0.6,3.0,3.9,2.8 ng,and the limits of detection were 2.2,1.0,0.4,1.4,0.3,1.0,2.0,1.4 ng,respectively.RSDs of precision tests were all lower than 2.0％.Only ethanol,methanol and methylbenzene were detected in reproducibility test,RSDs of their peak area were lower than 2.0％.The recoveries were 95.6％-104.9％ (RSD=3.3％,n=9),98.7％-102.0％ (RSD=1.1％,n=9),100.0％-103.1％ (RSD=1.1％,n=9),95.7％-104.4％ (RSD=3.0％,n=9),99.3％-104.4％ (RSD=1.7 ％,n=9),95.6％-102.2％ (RSD=2.6％,n=9),95.1％-103.3％ (RSD=2.6％,n=9),97.5％-103.3％ (RSD =1.7 ％,n =9),respectively.CONCLUSIONS:The method is sensitive and simple,and it is suitable for simultaneous determination of 8 residual organic solvents in esomerarazole magnesium raw material.
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Objective: To establish the capillary GC fingerprint of Guominxing Biyan Granules and give a new method for quality control. Methods: The capillary GC was used. The ingredients of common peaks were analyzed by FID and MS. The HP-5 Phenyl Methyl Siloxane (30 m×0.32 mm, 0.25 μm) was used for capillary column. The chromatography conditions were as follows: the temperature of inlet was 200℃ in splitless sampling, the detector temperature was 250℃, the column initial temperature was 50℃, 3℃/min rose to 140℃, keeping 2 min and 10℃/min rose to 200℃, keeping 2 min. Results: Capillary GC fingerprint of volatile oil in Allergic Rhinitis Particles was established. Twelve peaks were selected as the fingerprint peaks of Allergic Rhinitis Particles. The ingredients of common peaks were designated by GC-MS. The similarity between the fingerprint of 10 batches of Allergic Rhinitis Particles Samples were 0.90. Conclusion: The established capillary GC fingerprint has desirable precision, reproducibility, and stability, and can be applied to the quality control of Guominxing Biyan Granules.
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OBJECTIVE:To establish a method for determining residual solvents in Decitabine for injection. METHODS:Cap-illary GC method was adopted,and the contents of residual solvents were calculated by internal standard method. The column was capillary column Agilent DB-624,flame ionization detector was used with the temperature of 280 ℃ by temperature programming, and the temperature of injector was 230 ℃,nitrogen was used as the carrier gas,flow rate was 1.5 ml/min and the split ratio was 50:1,direct injection was used,and the sample size was 1 μl. RESULTS:The linear range was 0.100 3-2.507 mg/ml for ethanol , 0.101 3-2.532 mg/ml for ether,0.102 2-2.556 mg/ml for isopropanol,0.008 3-0.207 8 mg/ml for acetonitrile,0.012 4-0.309 3 mg/ml for methylene chloride,0.014 8-0.369 4 mg/ml for tetrahydrofuran,0.078 1-1.953 mg/ml for cyclohexane,0.024 9-1.250 mg/ml for toluene and 0.017 6-0.440 9 mg/ml for N,N-dimethylformamide(r≥0.999 2);RSDs of precision and reproducibility tests were lower than 2%;recovery was 96.70%-101.60%(RSD was 0.59%-1.82%,n=9). CONCLUSIONS:The method is simple,accurate and reproducible and suitable for determining the residual solvents in Decitabine for injection.
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OBJECTIVE:To establish a method for the determination of residuals of petroleum ether,ethanol,xylene and ace-tic acid in ecabet sodium crude drug. METHODS:Capillary GC was performed on the column of PGE-20M capillary column at the flow rate of 1.7 ml/min,detector was hydrogen flame ionization detector,carrier gas was nitrogen with high purity,column temper-ature was 45 ℃,maintaining 4 min,it increased to 80 ℃ with rate of 10 ℃/min,then increased to 135 ℃ with rate of 30 ℃/min,maintaining 3 min,the injection mode was direct injection,inlet temperature was 250 ℃,and the volume injection was 1.0 μl. RESULTS:The mass concentration was 0.050-1.952 g/L for petroleum ether,0.050-1.941 g/L for ethanol,0.024-0.948 g/L for xy-lene and 0.050-1.947g/L for acetic acid(r=0.999 1-0.999 7);RSDs of precision,stability and reproducibility tests were no more than 1.7%;recoveries were 99.3%-101.0%(RSD=0.7%,n=9),102.3%-103.7%(RSD=0.4%,n=9),101.2%-102.1%(RSD=0.3%,n=9) and 100.3%-102.2%(RSD=0.6%,n=9),respectively. CONCLUSIONS:The method is simple and accurate,and can be used for the control of residual of organic solvents in ecabet sodium crude drug.
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Objective:To establish a method for the determination of 8 residual organic solvents in tolterodine tartrate by capillary GC. Methods: The determination of methanol, ethanol, acetonitrile, acetone, ethyl acetate, trichloromethane and tetrahydrofuran in tolterodine tartrate dissolved in the solution of N, N-dimethylformamide-water ( 1∶ 4 ) was carried out on a CP-sil 5CB ( 60. 0 m × 0. 32 mm,5μm)column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The flow rate of carrier gas was 1. 2 ml·min-1 . The column temperature was 120℃. The headspace vial temperature was 85℃ and the time was 30min. The determina-tion of pyridine in tolterodine tartrate dissolved in the solution of dimethylsulfoxide-sodium hydroxide (17∶13) was carried out on an HP-1(30. 0 m × 0. 53 mm,5 μm) column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column tem-perature was 80℃. The flow rate of carrier gas was 3. 0 ml·min-1 . The headspace vial temperature was 85℃ and the time was 30 min. Results:All peaks could be separated from each other under the chromatographic conditions. The linearity of the eight solvents was falrly good (r>0. 999). The average recovery was ranged from 86. 0% to 100. 2% with RSD of 1. 7%-3. 5% (n=9). The limit of detection was 0. 63, 0. 43, 0. 30, 0. 18, 0. 079, 0. 36, 0. 18 and 0. 89 μg·ml-1 , respectively. Conclusion:The methods can be applied in the determination of the eight residual organic solvents in tolterodine tartrate.
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Objective:To establish a capillary GC method for the determination of residual organic solvents in paclitaxel. Meth-ods:The standard solution and test solution was respectively injected into an HP-INNOWAX sillica capillary column by headspace in-jection. The chromatograms were recorded with an FID. The injection port and detector temperature was 250℃ and 300℃, respective-ly, the initial column temperature was kept at 35℃ for 5 min, and then was risen to 260℃ at the rate of 25℃/min. Results:The four residual organic solvents could be separated completely. The resolution and sensitivity were acceptable. Conclusion: The method is proved to be simple, rapid, sensitive and reliable, and can be used in the determination of residual organic solvents in paclitaxel.
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Objective:To establish a determination method for 8 residual organic solvents in spironolactone by capillary GC. Methods:The determination of methanol, ethanol, acetone and tetrahydrofuran in spironolactone dissolved in dimethyl sulfoxide was carried out on a DB-624 column. The inlet temperature was 200℃ and the FID detector temperature was 250℃. The constant pressure was 2. 5psi. The column temperature was raised by program. The vial temperature was 85℃ and the time was 30min. The determination of triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide in spironolactone dissolved in chloroform was carried out on an HP-1 column. The inlet temperature was 220℃ and the FID detector temperature was 250℃. The column temperature was raised by program. The flow rate of carrier gas was 3. 0ml·min-1. Results: All peaks could be separated from each other with promising resolution. The linearity of the eight solvents was fairly good(r > 0. 999). The average recovery ranged from 90. 9%-94. 3% with RSD of 1. 1%-3. 3% (n = 9). The limit of detection for methanol, ethanol, acetone, tetrahydrofuran, triethylamine, pyridine, N,N-dimethylformamide and dimethyl sulfoxide was 0. 60, 0. 67, 0. 20, 0. 15, 0. 64, 0. 36, 0. 89 and 0. 82 μg · ml-1 , respectively. Conclusion: The methods can be applied in the determination of 8 residual organic solvents in spironolactone.
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OBJECTIVE:To establish capillary GC method for the determination of residual organic solvents in artesunate,such as methanol and ethyl acetate.METHODS:Capillary GC was adopted and the temperature of flame ionization detector was 250℃.RESULTS:The linear range were 0.03～0.605 mg?mL-1 for methanol(r=0.999 8) and 0.05～1.002 mg?mL-1 for ethyl acetate(r=0.999 7).The average recovery rates were 98.7% for methanol(RSD=3.0%) and 99.1% for ethyl acetate(RSD=2.1%).Only the ethyl acetate was detected in samples.CONCLUSION:Established method is simple and accurate for the content determination of residual organic solvents in artesunate.
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AIM: To establish a method for detecting the residual solvents in protopanaxdiol. METHODS: Capillary GC with HP-PLOT-Q column (30 m ? 0. 53 mm ? 1. 0 ?m) was used to determine residual in protopanaxdiol. N,N-dimethyl-acetamide as solvent media,FID detector and nitrogen as the carrier gas. RESULTS: There was a good linearity at the experimental concentration (r = 0. 999 96-0. 999 99),the RSD of precision was less than 6. 0 % . The spotting recovery of the 3 residul,including methol,ethyl acetate and n-butanol,was in the range of 98. 2%-102. 2% ,and its’RSD was 1. 1%-2. 4% . CONCLUSION: The method is simple,accurate and of high sensitivity,can be used for the determination of residual solvents in protopanaxdiol.
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AIM:To develop a capillary GC method for determining six components in Heiguidou Oil,?-pinene,eucalyptol,borneol,methyl salicylate,cinnamia aldehyde and eugenol. METHODS:GC was applied to quantitative analysis. Chromatographic conditions consisted of PEG-20M(30 m?0.25 mm?0.25 ?m),flame ionization detector(FID),and programmed temperature; initiation temperature was at 80 ℃ for 7 min; the rate of temperature was 15℃/minute,final temperature was at 180 ℃ for 10 min,bypass rate was 50 ∶1. The sample dissolved in absolute alcohol. The external standard was used. RESULTS:The standard curves of conclusion ?-pinene,eucalyptol,borneol,methyl salicylate,cinnamia aldehyde and eugenol were linear within the ranges of 0.322-32.150 mg/mL,0.202 -20.215 mg/mL,0.126-12.630 mg/mL,0.633-63.290 mg/mL,0.174-17.390 mg/mL,0.633-63.290 mg/mL and 0.203-20.255 mg/mL,respectively.RSD were 0.83%,0.48%,0.48%,0.31%,and 0.53 %,respectively. CONCLUSION:The established method is accurate and it can be applied to the simulta-neous assay of six components.